Nitrogen → 1-Chloro-6-methoxyphthalazine

HRID 2268828노트

반응식

HRID 2268828 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][N:7]=[CH:6]2.N#N.P(Cl)(Cl)([Cl:18])=O>C(#N)C>[Cl:18][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[N:7][N:8]=1

참가 물질

5

반응물 3

HCID 947NitrogenHCID 24813Phosphorus oxychlorideHCID 122985436-Methoxyphthalazin-1-ol

생성물 1

HCID 183816081-Chloro-6-methoxyphthalazine수율 98.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 6-methoxy-2H-phthalazin-1-one (6.4 g, 36.3 mmoles), prepared as described in example 3, in acetonitrile (65 ml) under stirring and dry N2 at room temperature, was dropwise added with phosphorous oxychloride (6.8 ml, 73 mmoles), then the mixture was refluxed. After 3 hours the mixture was concentrated, taken up in water, neutralised with NaHCO3 and extracted more times with CH2Cl2. The organic phases were washed with water, anhydrified and concentrated to give 6.94 g of the title compound (yield: 98.3%). m.p.: 181-183° C.

후처리

  1. customprepared
  2. temperaturethe mixture was refluxed
  3. concentrationAfter 3 hours the mixture was concentrated
  4. extractionextracted more times with CH2Cl2
  5. washThe organic phases were washed with water, anhydrified
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-29f621a189f4445b9ecb0371d7a99b92
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329370B1

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